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1.
Hui‐Jie Cheng Katrin Lippe Edwin Kroke Jörg Wagler Gerrit W. Fester Ya‐Li Li Marcus R. Schwarz Tatyana Saplinova Stefanie Herkenhoff Vladislav Ischenko Jörg Woltersdorf 《应用有机金属化学》2011,25(10):735-747
Polymeric Si/C/O/N xerogels, with the idealized polymer network structure comprising [Si O Si(NCN)3]n moieties, were prepared by reactions of hexachlorodisiloxane (Cl3Si O SiCl3) with bis(trimethylsilyl)carbodiimide (Me3Si NCN SiMe3, BTSC). NMR and FTIR spectra indicate the existence of ‐NCN‐ and Si O Si‐ units in the xerogels and also in the ceramic materials obtained upon pyrolysis. The feasibility of this reaction protocol was confirmed on the molecular level by the deliberate synthesis of the macrocyclic compound [SiPh2 O SiPh2(NCN)]2, the crystal structure and spectroscopic data of which are reported. The influence of pyridine as a catalyst for the cross‐linking reaction was studied. The degree of cross‐linking increased within the polymers with the addition of pyridine. It was shown by the reaction of hexachlorodisiloxane with excess pyridine that the latter appears to activate only one out of the two ‐SiCl3 moieties under formation of hexacoordinated silicon compounds. The crystal structure of Cl3Si O SiCl3(pyridine)2 is presented. Quantum chemical calculations are in support of this adduct being a potential intermediate in the pyridine catalyzed sol–gel process. The ceramic yield after pyrolysis of the Si/C/O/N‐xerogels at 1000 °C, which reaches values up to 50%, was found to depend on the aging protocol (time, temperature), whereas no correlation was found with the amount of pyridine added for xerogel synthesis. The Si/C/N/O‐ceramics obtained after pyrolysis at 1000 °C under NH3 are completely amorphous. Chemically they have to be considered as hybrids between an ideal [SiOSi(NCN)3]n network and glass‐like Si2N2O. The products are mesoporous with closed pores and a broad pore size distribution. Copyright © 2011 John Wiley & Sons, Ltd. 相似文献
2.
Josef Pola Anna Galíkov Zdenk Bastl Jan ubrt Karel Vacek Jií Brus Akihiko Ouchi 《应用有机金属化学》2006,20(10):648-655
Megawatt ArF laser photolysis of gaseous methyldisilazanes [(CH3)nH3?nSi]2NH (n = 2, 3) in excess of Ar yields hydrocarbons (major volatile products), methylsilanes (minor volatile products) and allows chemical vapour deposition of solid amorphous Si/C/O/N/H powder containing Si? X (X? C, H, O, N) bonds. The incorporation of O is due to a high reactivity of the primarily formed products towards air moisture. The resulting solid materials possess nanometer‐sized texture and high specific area, contain Si‐centered radicals and anneal under argon to silicon oxycarbonitride, whose structure is described as a network of O‐ and N‐interconnected Si and C atoms. Copyright © 2006 John Wiley & Sons, Ltd. 相似文献
3.
Thermal silazane cleavage of dichloroboryldisilylamines (SiClmMe3?m)N(SiMe3)(BCl2) (1: m = 1; 2: m = 2) at 196 °C leads to the borazine derivates [(SiClmMe3?m)NB(ClnMe1?n)]3 (3: m = 1, n = 0.185; 4: m = 2, n = 0.111) characterized by NMR and IR spectroscopy and mass spectrometry. Single‐crystal X‐ray diffraction structure analyses reveal (BN)3 units with unusual twisted boat conformations in both compounds. Additionally, more detailed studies are done to clear up the function of the by‐products (SiClmMe3?m)N(SiClMe2)(BClMe) formed during the cyclization step leading to asymmetrically boron substituted borazine derivatives. The single‐source precursors 3 and 4 were cross‐linked with methylamine producing polymers 3P and 4P, which were transformed into black amorphous materials with ceramic yields of 20.8 % and 50.3 %, respectively. Ceramic 4C (Si1.00B0.98 N2.55 C1.37O0.05) was further investigated by 11B and 29Si magic angle spinning (MAS) NMR spectroscopy. A combined study of high‐temperature TG analyses and X‐ray powder diffraction analyses confirms the thermal stability of 4C up to 1670 °C. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
4.
《Magnetic resonance in chemistry : MRC》2002,40(11):723-728
The C(2) isotropic chemical shift values in solid‐state CP/MAS 13C NMR spectra of conformational polymorphs Form I (δ 28.5) and III (δ 22.9) of (1S,4S)‐sertraline HCl ( 1 ) were correlated with a γ‐gauche effect resulting from the respective 162.6° antiperiplanar and 68.8° (+)‐synclinal C(2)? C(1)? N? CH3 torsion angles as measured by X‐ray crystallography. The similarity of the solution‐state C(2) chemical shifts in CD2Cl2 (δ 22.8) and DMSO‐d6 (δ 23.4) with that for Form III (and other polymorphs having C(2)? C(1)? N? CH3 (+)‐synclinal angles) strongly suggests that a conformational bias about the C(1)? N bond exists for 1 in both solvents. This conclusion is supported by density functional theory B3LYP/6‐31G(d)‐calculated relative energies of C(1)? N rotameric models: (kcal) 0.00 [73.8 °C(2)? C(1)? N? CH3 torsion angle], 0.88 (168.7°), and 2.40 (?63.4°). A Boltzmann distribution of these conformations at 25 °C is estimated to be respectively (%) 80.3, 18.3, and 1.4. Copyright © 2002 John Wiley & Sons, Ltd. 相似文献
5.
Ke Li Xiao Ting Liu Yun Fei Zhang Donglei Liu Xin Yu Zhang Song Mei Ma Juan M. Ruso Zhenghua Tang Zhen Bin Chen Zhen Liu 《先进技术聚合物》2019,30(1):86-93
In this work, the relationships between catalytic performances of penicillin G acylase (PGA) and the molar ratio of carrier, thermo‐sensitive tri‐block polymer, poly (N,N‐diethylacrylamide‐b‐ β‐hydroxyethyl methacrylate‐b‐glycidyl methacrylate) (PDEA‐b‐PHEMA‐b‐PGMA) were studied firstly, and result documented the optimal molar ratio was nDEA:nHEMA:nGMA = 100:47:24, which presented a suitable lower critical solution temperature (LCST) of 35°C and the activity retention ratio of 80.62% (±0.50%). Based on the suitable carrier, immobilization conditions were investigated and optimized. When pH of solution, concentration of PGA, immobilized time, and immobilization temperature were 8.0, 1/10 (m/v), 16 hours, and 36°C, respectively, enzyme loading capacity (L), enzyme activity (Ea), and activity retention ratio (Ar) of PGA arrived at the highest value of 21 223 U, 16 199 U/g, and 93.50% (±0.50%), respectively. Besides, the response rate (Rr) of immobilized PGA was the same as free PGA, the reusable stability (Rs) was 77.00% (±1.00%) after using for 11 times, which indicated that the carrier has better compatibility with L, Ar, Rs, and Rr. 相似文献
6.
Makiko Seno Makoto Hasegawa Tomohiro Hirano Tsuneyuki Sato 《Journal of polymer science. Part A, Polymer chemistry》2005,43(23):5864-5871
Trimethoxyvinylsilane (TMVS) was quantitatively polymerized at 130 °C in bulk, using dicumyl peroxide (DCPO) as initiator. The polymerization of TMVS with DCPO was kinetically studied in dioxane by Fourier transform near‐infrared spectroscopy. The overall activation energy of the bulk polymerization was estimated to be 112 kJ/mol. The initial polymerization rate (Rp) was expressed by Rp = k[DCPO]0.6[TMVS]1.0 at 120 °C, being closely similar to that of the conventional radical polymerization involving bimolecular termination. The polymerization system involved electron spin resonance (ESR) spectroscopically observable polymer radicals under the actual polymerization conditions. ESR‐determined apparent rate constants of propagation and termination were 13 L/mol s and 3.1 × 104 L/mol s at 120 °C, respectively. The molecular weight of the resulting poly(TMVS)s was low (Mn = 2.0–4.4 × 103), because of the high chain transfer constant (Cmtr = 4.2 × 10?2 at 120 °C) to the monomer. The bulk copolymerization of TMVS (M1) and vinyl acetate (M2) at 120 °C gave the following copolymerization parameters: rl = 1.4, r2 = 0.24, Q1 = 0.084, and e1 = +0.80. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 5864–5871, 2005 相似文献
7.
Characterization of the electronic structure and thermal stability of HfO2/SiO2/Si gate dielectric stack 下载免费PDF全文
X‐ray photoelectron spectroscopy was used to investigate thermal stability of HfO2 on SiO2/Si substrate prepared by atomic layer deposition, followed by annealing at different temperature. Hf silicate and Hf silicide are formed at the interface of HfO2 and SiO2 during deposition. The Hf silicide disappears, while the amount of the Hf silicate is intensified after post‐deposition annealing treatment at 400 °C. Phase separation of the Hf silicate layer occurs when the annealing temperature is over 400 °C, resulting in the Hf silicate decomposition into Si and Hf oxides. Moreover, crystallization at high temperature leads to grain boundaries formation, which deteriorates the gate leakage current, as observed by the electrical measurements. The similar annealing temperature dependence of both internal electric field and the amount of Hf silicate implies that the Hf silicate plays a key role in building up the internal electric field, which is attributed to generation of oxygen vacancies (Vo) in the Hf silicate layer. Copyright © 2017 John Wiley & Sons, Ltd. 相似文献
8.
《先进技术聚合物》2018,29(2):934-940
A novel heat‐curable silicone rubber (MCSR/Si‐PAMAM) was prepared by using siloxane polyamidoamine (Si‐PAMAM) dendrimers as cross‐linkers and polysiloxane containing γ‐chloropropyl groups as gums. The chemical cross‐linking occurs through the reaction between Si‐PAMAM dendrimers and polysiloxane containing γ‐chloropropyl groups. The effect of various amounts of cross‐linkers on mechanical properties of MCSR/Si‐PAMAM was discussed in this paper. MCSR/Si‐PAMAM exhibits favorable mechanical properties with a tensile strength of 10.06 MPa and a tear strength of 47.9 kN/m when the molar ratio r of [N‐H]/[CH2CH2CH2Cl] is 1:1. These excellent mechanical properties can be attributed to the formation of concentrative cross‐linking from Si‐PAMAM dendrimers in the cross‐linking networks, along with the introduction of Si–O–Si units in the internal structure of dendrimers. The introduction of Si–O–Si units reduces the steric hindrance of molecular structure, which facilitates the N–H bonds in the interior layers of dendrimers to react with γ‐chloropropyl groups. In addition, thermogravimetric analysis results indicate that MCSR/Si‐PAMAM is thermally stable even at high temperatures in a nitrogen atmosphere. Differential scanning calorimetry analysis reveals that the glass transition peak of MCSR/Si‐PAMAM is not identified in the temperature range −150 to −30°C, only a melting endothermic peak at −40°C. 相似文献
9.
Controlled coammonolysis of elementalkylamides in aprotic organic solvents at low temperatures have been shown to result in the formation of polyazanes. The synthetic procedure developed may be addressed as “sol‐gel‐route in the ammono system”. Pyrolysis of these novel polymer precursors gave access to multinary nitrides. For the model systems Si(NHMe)4/B(NMe2)3, Si(NHMe)4/Ti(NMe2)4, and Si(NHMe)4/Ta(NMe2)5 polymeric boro‐, titano and tantalosilazanes were obtained. Pyrolysis in ammonia at 1000 °C yielded amorphous silicon boron nitride, silicon titanium nitride and silicon tantalum nitride powders; further heating of the nitride powders at 1500 °C in nitrogen atmosphere led to the formation of partly crystalline composites of α‐Si3N4 and amorphous silicon boron nitride for the Si/B/N system, a composite of finely dispersed TiN and amorphous silicon titanium nitride for the Si/Ti/N system, and crystalline TaN and amorphous silicon nitride for the Si/Ta/N system. Furthermore, the structure and pyrolysis chemistry of the polymeric intermediates, as well as the morphology of the pyrolysis products, were studied by NMR, MAS‐NMR, FT‐IR, DTA‐TG‐MS, XRD, SEM, EDX and elemental analyses. 相似文献
10.
Lipase‐catalyzed ring‐opening bulk polymerizations of 3(S)‐sec‐butylmorpholine‐2,5‐dione (BMD) were investigated. Selected commercial lipases were screened as catalysts for BMD polymerization at 110°C. Polymerizations catalyzed with 10 wt.‐% of lipase PPL and PC result in BMD conversions of about 70% and in molecular weights of the products ranging from 5 500 to 10 700. Lipases MJ, CR and ES showed lower catalytic activities for the polymerization of BMD. Poly(3‐sec‐butylmorpholine‐2,5‐dione) has a carboxylic acid group at one end and a hydroxy group at the other end. During the polymerization racemization of the isoleucine residue takes place. Lipase PPL was selected for a more detailed study. The apparent rate of polymerization increases with increasing PPL concentration when the polymerization temperature is 110°C. When the PPL concentration is 5 and 10 wt.‐% with respect to the monomer, a conversion of about 70% is reached after 5 d and 3 d, respectively, while for a PPL concentration of 1 wt.‐% the conversion is less than 7% even after 6 d. High concentrations of PPL (10 wt.‐%) result in high Mn values (< 4 d). The highest molecular weight poly(BMD), Mn = 19 900, resulted from a polymerization conducted at 120°C with 5 wt.‐% PPL for 6 d. The general trend observed by varying the polymerization temperature is as follows: (i) monomer conversion and Mn increase with increasing reaction temperature from 110 to 125°C, (ii) monomer conversion and Mn decrease with an increase in reaction temperature from 125 to 130°C. Water content was found to be an important factor that controls both the conversion and the molecular weight. With increasing water content, enhanced polymerization rates are achieved while the molecular weight of poly(BMD) decreases. 相似文献
11.
《应用有机金属化学》2017,31(12)
Amorphous silicon carbonitride (a‐SiCN) films were produced by remote nitrogen plasma chemical vapour deposition (RP‐CVD) from bis(dimethylamino)methylsilane precursor. The effect of substrate temperature (T S) on the kinetics of RP‐CVD, chemical structure, surface morphology and some properties of the resulting films is reported. The T S dependence of film growth rate implies that RP‐CVD is an adsorption‐controlled process. Fourier transform infrared spectroscopic examination revealed that an increase in T S from 30 to 400°C involves the elimination of organic moieties from the film and the formation of Si─C and Si─N network structure. The films were characterized in terms of their surface roughness and basic physical and optical properties, such as density and refractive index, respectively. Reasonably good relationships between the structural parameters represented by relative integrated intensity of infrared absorption bands from the Si─C and Si─N bonds (controlled by T S) and the film properties are determined. Due to their small surface roughness, high density and high refractive index, the a‐SiCN films produced at T S ≥ 350°C would seem to be useful protective coatings for metals and optical devices. 相似文献
12.
A Systematic Study of Structure and E−H Bond Activation Chemistry by Sterically Encumbered Germylene Complexes 下载免费PDF全文
Matthew Usher Dr. Andrey V. Protchenko Dr. Arnab Rit Dr. Jesús Campos Dr. Eugene L. Kolychev Dr. Rémi Tirfoin Prof. Dr. Simon Aldridge 《Chemistry (Weinheim an der Bergstrasse, Germany)》2016,22(33):11685-11698
A series of new germylene compounds has been synthesized offering systematic variation in the σ‐ and π‐capabilities of the α‐substituent and differing levels of reactivity towards E?H bond activation (E=H, B, C, N, Si, Ge). Chloride metathesis utilizing [(terphenyl)GeCl] proves to be an effective synthetic route to complexes of the type [(terphenyl)Ge(ERn)] ( 1 – 6 : ERn=NHDipp, CH(SiMe3)2, P(SiMe3)2, Si(SiMe3)3 or B(NDippCH)2; terphenyl=C6H3Mes2‐2,6=ArMes or C6H3Dipp2‐2,6=ArDipp; Dipp=C6H3iPr2‐2,6, Mes=C6H2Me3‐2,4,6), while the related complex [{(Me3Si)2N}Ge{B(NDippCH)2}] ( 8 ) can be accessed by an amide/boryl exchange route. Metrical parameters have been probed by X‐ray crystallography, and are consistent with widening angles at the metal centre as more bulky and/or more electropositive substituents are employed. Thus, the widest germylene units (θ>110°) are found to be associated with strongly σ‐donating boryl or silyl ancillary donors. HOMO–LUMO gaps for the new germylene complexes have been appraised by DFT calculations. The aryl(boryl)‐germylene system [ArMesGe{B(NDippCH)2}] ( 6 ‐Mes), which features a wide C‐Ge‐B angle (110.4(1)°) and (albeit relatively weak) ancillary π‐acceptor capabilities, has the smallest HOMO–LUMO gap (119 kJ mol?1). These features result in 6 ‐Mes being remarkably reactive, undergoing facile intramolecular C?H activation involving one of the mesityl ortho‐methyl groups. The related aryl(silyl)‐germylene system, [ArMesGe{Si(SiMe3)3}] ( 5 ‐Mes) has a marginally wider HOMO–LUMO gap (134 kJ mol?1), rendering it less labile towards decomposition, yet reactive enough to oxidatively cleave H2 and NH3 to give the corresponding dihydride and (amido)hydride. Mixed aryl/alkyl, aryl/amido and aryl/phosphido complexes are unreactive, but amido/boryl complex 8 is competent for the activation of E?H bonds (E=H, B, Si) to give hydrido, boryl and silyl products. The results of these reactivity studies imply that the use of the very strongly σ‐donating boryl or silyl substituents is an effective strategy for rendering metallylene complexes competent for E?H bond activation. 相似文献
13.
Single-step sol–gel deposition was attempted for realizing submicron thick, (001) oriented Pb(Zr0.53Ti0.47)O3 (PZT) thin films, using an alkoxide solution containing polyvinylpyrrolidone (PVP). A solution of molar composition, Pb(NO3)2:Zr(OC3H7
n)4:Ti(OC3H7
i)4:PVP:H2O:CH3COCH2COCH3:CH3OC2H4OH:C3H7
nOH = 1.1:0.53:0.47:0.5:5:0.5:22:0.98, was prepared as a coating solution. Gel films were prepared on Pt(111)/TiO2/SiO2/Si(100) substrates by spin-coating, and calcined at 350 °C and annealed at 650 °C either in an electric furnace or in a near-infrared
(IR) furnace. When calcined in the near-IR furnace, the films became (001) oriented on annealing. When calcined in the electric
furnace, on the other hand, the films became randomly oriented on annealing. These observations indicate that the heating
the gel films from the substrate side in the calcination step at 350 °C induces crystallographic orientation in the annealing
step at 650 °C. The effects of the heating methods on the thermal decomposition of the gel films, and the microstructure and
dielectric properties of the fired films were studied. Finally 0.4 μm thick, (001) oriented PZT films could be successfully
prepared by non-repetitive, single-step deposition. The oriented film thus obtained had the remnant polarization 2P
r of 39 μC/cm2 and the dielectric constant ε′ of 960 ± 169. 相似文献
14.
Preparation and thermal stability of fluoroalkyl end‐capped vinyltrimethoxysilane oligomeric silica/boric acid nanocomposites‐encapsulated a variety of low molecular weight organic compounds 下载免费PDF全文
Yuta Aomi Masakazu Nishida Hideo Sawada 《Journal of polymer science. Part A, Polymer chemistry》2016,54(24):3835-3845
Fluoroalkyl end‐capped vinyltrimethoxysilane oligomer [RF‐(VM)n‐RF] reacted with boric acid to afford the corresponding fluorinated oligomeric silica/boric acid nanocomposite [RF‐(VM? SiO2)n‐RF/B(OH)3] fine particles with mean diameter: 36–105 nm. The obtained RF‐(VM? SiO2)n‐RF/B(OH)3 nanocomposites were applied to the encapsulation of low molecular weight organic compounds such as diphenylsilanediol, 1,1′‐bi‐2‐naphthol, 4,4′‐biphenol, bisphenol A, bisphenol F, bisphenol AF, biphenyl, dibenzyl, and pentaerythritol into these nanocomposite cores to provide the corresponding fluorinated oligomeric silica/boric acid nanocomposites—encapsulated these organic molecules. Interestingly, the obtained nanocomposites were found to exhibit no weight loss behavior corresponding to the contents of these guest molecules even after calcination at 800 °C, although these nanocomposites were isolated through no purification process. The RF‐(VM? SiO2)n‐RF nanocomposites—encapsulated these organic guest molecules were prepared under similar conditions. However, it was demonstrated that these nanocomposites can provide the clear weight loss corresponding to the contents of these guest molecules in the nanocomposites after calcination at 800 °C. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2016 , 54, 3835–3845 相似文献
15.
ludk Toman Miroslav Janata Jií Spv
ek Barbora Dvonkov Petra Ltalov Petr Vl
ek Antonín Sikora Jií Michlek Michal Pekrek 《Journal of polymer science. Part A, Polymer chemistry》2006,44(9):2891-2900
Amphiphilic polymer networks consisting of hydrophilic poly(2‐hydroxyethyl methacrylate) (PHEMA) and hydrophobic polyisobutylene (PIB) chains were synthesized from a cationic copolymer of isobutylene (IB) and 3‐isopropenyl‐α,α‐dimethylbenzyl isocyanate (IDI) prepared at ?50 °C in dichloromethane in conjunction with SnCl4. The isocyanate groups of this random copolymer, PIB(NCO)n, were subsequently transformed in situ to methacrylate (MA) groups in the dibutyltin dilaurate‐catalyzed reaction with 2‐hydroxyethyl methacrylate (HEMA) at 30 °C. The resulting PIB(MA)n with number–average molecular weight 8200 and average functionality Fn ~ 4 per chain was in situ copolymerized radically with HEMA at 70 °C, giving rise to the amphiphilic networks containing 41 and 67 mol % HEMA. PHEMA–PIB network containing 43 mol % HEMA was also prepared by radical copolymerization of PIB(MA)n precursor with HEMA using sequential synthesis. An amphiphilic nature of the resulting networks was proved by swelling in both water and n‐heptane. PIB(NCO)n and PIB(MA)n were characterized by FTIR spectroscopy, SEC and the latter also by 1H NMR spectroscopy. Solid state 13C NMR spectroscopy was used for characterization of the resulting PHEMA–PIB networks. Whereas single glass‐transition temperature, Tg = ?67.4 °C, was observed for the rubbery crosslinked PIB prepared by reaction of PIB(NCO)n with water, the PHEMA–PIB networks containing 67 and 41 mol % HEMA showed two Tg's: ?70.4 and 102.7 °C, and ?63 and 107.2 °C, respectively. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 2891–2900, 2006 相似文献
16.
Owing to steric congestion in i‐Pr2(2,4,6‐i‐Pr3C6H2)SiF, the geometry at the Si atom deviates slightly from ideal tetrahedral geometry with an increased C? Si? C angle of 119.02(9)° and elongated Si? C and Si? F bond distances. Copyright © 2005 John Wiley & Sons, Ltd. 相似文献
17.
Christoph Frster Daniel Siebler Katja Heinze 《Acta Crystallographica. Section C, Structural Chemistry》2010,66(9):m235-m237
The title compund, [Fe(C5H6N)(C7H7O2)], features one strong intermolecular hydrogen bond of the type N—H...O=C [N...O = 3.028 (2) Å] between the amine group and the carbonyl group of a neighbouring molecule, and vice versa, to form a centrosymmetric dimer. Furthermore, the carbonyl group acts as a double H‐atom acceptor in the formation of a second, weaker, hydrogen bond of the type C—H...O=C [C...O = 3.283 (2) Å] with the methyl group of the ester group of a second neighbouring molecule at (x, −y − , z − ). The methyl group also acts as a weak hydrogen‐bond donor, symmetry‐related to the latter described C—H...O=C interaction, to a third molecule at (x, −y − , z + ) to form a two‐dimensional network. The cyclopentadienyl rings of the ferrocene unit are parallel to each other within 0.33 (3)° and show an almost eclipsed 1,1′‐conformation, with a relative twist angle of 9.32 (12)°. The ester group is twisted slightly [11.33 (8)°] relative to the cylopentadienyl plane due to the above‐mentioned intermolecular hydrogen bonds of the carbonyl group. The N atom shows pyramidal coordination geometry, with the sum of the X—N—Y angles being 340 (3)°. 相似文献
18.
E. Metwally A. Sh. Saleh S. M. Abdel-Wahaab H. A. El-Naggar 《Journal of Radioanalytical and Nuclear Chemistry》2010,286(1):217-221
The diamide N,N,N′,N′-tetraoctyldiglycolamide (TODGA) was synthesized and characterized. The prepared TODGA was applied for extraction of Ce(III)
from nitric acid solutions. The equilibrium studies included the dependencies of cerium distribution ratio on nitric acid,
TODGA, nitrate ion, hydrogen ion and cerous ion concentrations. Analysis of the results indicates that the main extracted
species is Ce(TODGA)2(NO3)3HNO3. The capacity of Ce loading is approximately 45 mmol/L for 0.1 M solution of TODGA in n-hexane. Finally, the thermodynamic parameters were calculated: K (25 °C) = 3.8 × 103, ΔH = −36.7 ± 1.0 kJ/mol, ΔS = −54.6 ± 3.0 J/K mol, and ΔG = −20.4 ± 0.1 kJ/mol. 相似文献
19.
Imre Miklós Szilágyi Eero Santala Mikko Heikkilä Marianna Kemell Timur Nikitin Leonid Khriachtchev Markku Räsänen Mikko Ritala Markku Leskelä 《Journal of Thermal Analysis and Calorimetry》2011,105(1):73-81
This article demonstrates how important it is to find the optimal heating conditions when electrospun organic/inorganic composite
fibers are annealed to get ceramic nanofibers in appropriate quality (crystal structure, composition, and morphology) and
to avoid their disintegration. Polyvinylpyrrolidone [PVP, (C6H9NO)
n
] and ammonium metatungstate [AMT, (NH4)6[H2W12O40]·nH2O] nanofibers were prepared by electrospinning aqueous solutions of PVP and AMT. The as-spun fibers and their annealing were
characterized by TG/DTA-MS, XRD, SEM, Raman, and FTIR measurements. The 400–600 nm thick and tens of micrometer long PVP/AMT
fibers decomposed thermally in air in four steps, and pure monoclinic WO3 nanofibers formed between 500 and 600 °C. When a too high heating rate and heating temperature (10 °C min−1, 600 °C) were used, the WO3 nanofibers completely disintegrated. At lower heating rate but too high temperature (1 °C min−1, 600 °C), the fibers broke into rods. If the heating rate was adequate, but the annealing temperature was too low (1 °C min−1, 500 °C), the nanofiber morphology was excellent, but the sample was less crystalline. When the optimal heating rate and
temperature (1 °C min−1, 550 °C) were applied, WO3 nanofibers with excellent morphology (250 nm thick and tens of micrometer long nanofibers, which consisted of 20–80 nm particles)
and crystallinity (monoclinic WO3) were obtained. The FTIR and Raman measurements confirmed that with these heating parameters the organic matter was effectively
removed from the nanofibers and monoclinic WO3 was present in a highly crystalline and ordered form. 相似文献
20.
The spreading behaviour of binary and ternary equimolar mixtures of siloxane surfactants of general formula [(CH3)3SiO]2CH3Si(CH2)3 (OCH2CH2) nOCH3, n = 3–9, has been investigated. The mixtures show a pronounced temperature dependence on the initial spreading rate. Mixtures imitating the average oligoethylene glycol chain length n = 5 are the fastest spreaders at 15 °C. At 23 °C and 40 °C these mixtures spread fastest sucking n = 6 and n = 8, respectively. For a given average chain length an increasing length difference between the components of the binary mixtures reduces the initial spreading rate. Nevertheless, substantial differences between the phase transition temperature Tc from the lamellar phase (Lα) into the two‐phase state (2Φ) and the actual spreading temperature are tolerated. A clear relation between phase transition temperature Tc and initial spreading rate does not exist. Copyright © 1999 John Wiley & Sons, Ltd. 相似文献